1、Designation: E322 12Standard Test Method forAnalysis of Low-Alloy Steels and Cast Irons by WavelengthDispersive X-Ray Fluorescence Spectrometry1This standard is issued under the fixed designation E322; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、 case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the X-ray fluorescence spectro-metric analysis of low-alloy ste
3、els and cast irons for thefollowing elements in the ranges indicated:Elements Mass Fraction Range, %Manganese 0.20 to 1.50Nickel 0.10 to 1.00Chromium 0.10 to 1.00Molybdenum 0.04 to 0.40Copper 0.05 to 0.30Vanadium 0.03 to 0.25NOTE 1These mass fraction ranges can be extended by the use ofsuitable refe
4、rence materials. The detection limit for the elements is lowerthan the listed minimum value. The ranges represent the actual levels atwhich this test method was tested.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of
5、 the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE350 Test Method
6、s for Chemical Analysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE351 Test Methods for Chemical Analysis of Cast IronAll TypesE882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE1361 Guide for Correction of Interelement Ef
7、fects inX-Ray Spectrometric AnalysisE1621 Guide for X-Ray Emission Spectrometric Analysis3. Terminology3.1 For definition of terms used in this test method, refer toTerminology E135.4. Summary of Test Method4.1 The sample is finished to a clean, uniform surface, andthen irradiated by an X-ray beam o
8、f high energy. The second-ary X rays produced are dispersed by means of a crystal and theintensities are measured by a detector at selected wavelengths.The results are obtained by relating measured intensities to anappropriate calibration curve.5. Significance and Use5.1 This test method is comparat
9、ive and intended for use asa routine method to test materials for compliance with com-positional specifications. It is assumed that all who use this testmethod will be trained analysts capable of performing commonlaboratory procedures skillfully and safely. It is expected thatwork will be performed
10、in a properly equipped laboratoryunder appropriate quality control practices, such as thosedescribed in Guide E882.6. Apparatus6.1 Specimen Preparation Equipment:6.1.1 Disk or Belt Sander, capable of providing test speci-mens with a uniform, clean surface finish, or other equivalentfinishing device.
11、6.2 Excitation Source:6.2.1 X-ray Generator, with a full-wave rectified powersupply, or constant potential power supply.6.2.2 X-ray Tube, with a high-purity tungsten target. Othertargets may be used provided they produce data that meets theprecision and bias in Section 14.6.3 Spectrometer:1This test
12、 method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and is the directresponsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Aug. 1, 2012. Published September 2012. Originallyapproved in 1967. L
13、ast previous edition approved in 2004 as E322 96 (2004).DOI: 10.1520/E0322-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page on
14、the ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.3.1 Analyzing Crystal, lithium fluoride LiF(200), flat orcurved having a 2d spacing of 0.40276 nm; or LiF(220), flat orcurved having a 2d spacing of 0.28473 nm.6.3.2
15、CollimationProvide appropriate collimation toachieve the required resolution. For curved optics, no collima-tion is required; the use of entrance and exit slits might berequired to reduce the intensity of background radiation.6.3.3 GoniometerA goniometer that provides an angularscan from 10 2 u to 1
16、48 2 u. Or alternatively, fixed channelsfor the analytes of interest, given in the scope of the method.6.3.4 Detectors, gas-filled proportional counters or scintil-lation counter. Other detectors may be used provided theyproduce data that meets the precision and bias in Section 14.6.4 Measuring Unit
17、An electronic circuit panel capable ofamplifying, counting, or integrating pulses received from thedetector tube. In addition, a pulse height analyzer should beavailable for pulse energy discrimination if needed. Goodprecision and accuracy have been obtained without the use ofa pulse height analyzer
18、.7. Reference Materials7.1 Certified Reference MaterialsLow-alloy steel and castiron certified reference materials are commercially availablefrom a number of sources.7.2 Reference MaterialsLow-alloy steel and cast ironreference materials can be used. They should be analyzed andthoroughly evaluated i
19、n accordance with Test Methods E350and E351.8. Hazards8.1 U.S Nuclear Regulatory standards for ionizing radiationas found in the Code of Federal Regulations 10 CFR Part 19,“Notices, Instructions and Reports to Workers: Inspection andInvestigations” and 10 CFR Part 20, “Standards for ProtectionAgains
20、t Radiation”3shall be observed at all X-ray emissionspectrometer installations in the U.S. It is also recommendedthat operating and maintenance personnel follow the guidelinesof safe operating procedures given in similar handbooks onradiation safety.8.2 Exposure to excessive quantities of high energ
21、y radia-tion such as those produced by X-ray spectrometers is injuriousto health. The operator should take appropriate actions to avoidexposing any part of their body, not only to primary X-rays, butalso to secondary or scattered radiation that might be present.The X-ray spectrometer should be opera
22、ted in accordance withthe regulations governing the use of ionizing radiation. Manu-facturers of x-ray fluorescence spectrometers generally buildappropriate shielding/safety interlocks into x-ray equipmentduring manufacturing which minimize the risk of excessiveradiation exposure to operators. Opera
23、tors should not attemptto bypass or defeat these safety devices. Only authorizedpersonnel should service x-ray spectrometers.9. Preparation of Reference Materials and Specimens9.1 Prepare a clean, flat surface on the test specimen usingan appropriate sander equipped with 240 grit or finer aluminumox
24、ide abrasive paper. The abrasive paper shall have a greaterdiameter than the exposed specimen surface. If disks are usedthe disk radius shall be greater than the exposed specimensurface. The specimen shall be surfaced using the same gritpaper as was used to prepare the surface of the calibrants.Othe
25、r equivalent finish-machining methods may be used pro-vided the data produced meets the precision and bias in Section14.NOTE 2Any facets or imperfections in the flatness of the finishedsurface have been found to give marked changes in response.9.2 Resurface the reference materials as needed to elimi
26、nateoxidized surfaces.10. Preparation of Apparatus10.1 Prepare the apparatus as follows:Voltage, kV 50 (Note 3)Current, mA 40 (Note 3)Detector Select the detector (or detector combination)according to the manufacturers recommendationNOTE 3Different values for voltage and current may be used provided
27、they produce data that meets the precision and bias in Section 14.11. Excitation and Radiation Measurement11.1 ExcitationPlace the specimen into the instrument,taking care not to contaminate the specimen surface. Generatethe secondary fluorescence using the settings listed in Section10.11.2 Radiatio
28、n MeasurementsMake radiation measure-ment of the analytical lines listed in Table 1 using the settingslisted in Section 10.NOTE 4In Table 1, the listed degree 2 u peaks represent the theoreticalvalues for lithium fluoride crystals LiF(200) and LiF(220) with 2dspacings of 0.40267 nm and 0.28473 nm re
29、spectively.The actual goniom-eter setting for these peaks must be determined experimentally within eachlaboratory. Periodic checks to verify this setting are advisable.11.2.1 Obtain the radiation measurement for each element.Collect sufficient counts to produce the required statisticalprecision. Use
30、 the data in the following Table to determine theminimum number of counts required:Element Total CountsNickel 64 000Manganese 64 000Chromium 64 000Molybdenum 32 000Copper 32 000Vanadium 16 0003Available from the Nuclear Regulatory Commission, Public Document Room,Mail Stop:OWFN-1 F13, Washington, DC
31、 20555, (800) 397- 4209, or via email atPDR.Resourcenrc.gov, or via the website at www.nrc.gov.TABLE 1 Analytical PeaksElement LineWave-length,nmCrystal2u(Note 4)AlternativeCrystal2u forAlternativeCrystal(Note 4)Nickel Ka (K-L3) 0.1659 LiF(200) 48.61 LiF(220) 71.27Manganese Ka (K-L3) 0.2103 LiF(200)
32、 62.91 LiF(220) 95.20Chromium Ka (K-L3) 0.2291 LiF(200) 69.29 LiF(220) 107.11Molybdenum Ka (K-L3) 0.0710 LiF(200) 20.28 LiF(220) 28.90Copper Ka (K-L3) 0.1542 LiF(200) 44.96 LiF(220) 65.56Vanadium Ka (K-L3) 0.2505 LiF(200) 76.84 LiF(220) 123.17E322 122NOTE 5Larger numbers than the above listed total
33、counts have beenaccumulated within a reasonable counting time by various instruments.12. Calibration and Standardization12.1 CalibrationMake measurements on a sufficient num-ber of reference materials to establish the calibration curve.Prepare the calibration curves for each element by plotting thei
34、ntensity versus mass fraction values. Refer to Guide E1361andGuide E1621 for additional information relating to soundcalibration practices.12.2 StandardizationBefore testing samples, standardizethe spectrometer calibration following the manufacturers in-structions.13. Calculation13.1 The mass fracti
35、ons are determined from the preparedcalibration curves.14. Precision and Bias14.1 PrecisionPrecision data are shown in Table 2.14.2 BiasRepresentative bias data are shown in Table 3.14.2.1 It is unlikely that any results using this test methodwill deviate more than the maximum deviation shown in Tab
36、le3, provided the operating parameters are as specified.NOTE 6The analyst must verify the absence of or accurate correctionof interferences such as zirconium on molybdenum Ka, the absence of oraccurate correction of inter-element effects such as molybdenum andnickel on chromium, and the absence of d
37、ifferences due to metallurgicalhistory or condition of the sample.15. Keywords15.1 cast iron; low-alloy steel; spectrometric analysis; X-rayfluorescenceASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Us
38、ers of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed ever
39、y five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible techni
40、cal committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocke
41、n, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photoco
42、py the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 2 Precision DataAElementMass FractionRange, %Relative Standard Deviation,RSD %BManganese 0.52 to 1.41 0.60Nickel 0.23 to 0.79 0.83Chromium 0.21 to 0.86 0.88Molybdenum 0.05 to 0.35 1.02Copper 0.06 to 0.27 1.04Va
43、nadium 0.03 to 0.22 1.16AThe values were obtained by pooling data from five laboratories.BRelative standard deviation, RSD, in this method, is calculated as follows:RSD 5 100/X! = (d2/n 2 1!where:X= average mass fraction,d = difference of the determination from the mean, andn = number of determinati
44、ons.TABLE 3 Bias DataElementEstablishedValue,Amassfraction %Deviation ofX-ray ValueBfrom Estab-lished Value,relative %MaximumObservedDeviationfromEstablishedValue, massfraction %Manganese 0.6400.9101.1201.140.550.960.030.020.025Nickel 0.3250.5200.6951.420.230.070.010.0050.007Chromium 0.3500.5150.700
45、0.492.350.740.010.0150.03Molybdenum 0.1000.1950.2951.903.330.580.0050.0080.005Copper 0.0600.0800.1753.830.630.970.0050.0040.007Vanadium 0.0450.14512.440.680.010.008AThe samples used for this program are secondary standards whose values areaverages from chemical analyses performed by eight laboratories.BThese values were calculated from the total results reported from threeseparate days of study, and five participating laboratories.E322 123
